CN103803556B - A kind of dewatering nano silicon oxide hollow ball of organic decoration and preparation thereof - Google Patents
A kind of dewatering nano silicon oxide hollow ball of organic decoration and preparation thereof Download PDFInfo
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Abstract
The dewatering nano silicon oxide hollow ball of organic decoration and a preparation thereof, the Nano-meter SiO_2 of the organic decoration obtained with microemulsion method
2solid sphere presoma, with mineral acids such as hydrochloric acid for etching reagent, prepares hollow nano silicon ball by the mode of chemical corrosion.It can adopt general formula OgHS to represent, Og is methyl, ethyl, propyl group, vinyl, dodecyl, octyl group, hexadecyl, one or more in naphthyl, phenyl, trifluoro propyl, pentafluorophenyl group; Does is HS Hollow? Silica.It is even that this hollow ball has cavity, and specific surface is large, the features such as surface hydrophobicity, and at medicament slow release, catalytic carrier, gas storage, pollutes the aspects such as absorption and have broad application prospects.
Description
Technical field
The invention belongs to nano material, specifically a kind of dewatering nano silicon oxide hollow ball of organic decoration and preparation thereof.
Background technology
Nano hollow sphere material is at medicament slow release, and support of the catalyst, pollute absorption, atmosphere storage aspect has a wide range of applications.But nano-hollow ball major part synthesized is at present hydrophilic, and it is bad that hydrophilic characteristic makes it disperse in organic phase, oil phase bad dispersibility, limit its application.If it is dispersed that the hollow ball can preparing a kind of surface hydrophobicity oleophylic certainly will can increase its oil phase, expand its range of application.
Traditional method preparing nano-hollow ball comprises soft template method, hard template method, Kirkendall effect, and Galvanic reduces, Ostawald effect etc.In recent years, the method for selective corrosion due to its process simple, preparation amount is large and receive much concern.These methods normally utilize the surface of solid sphere different with the structure of kernel and prepare.In conjunction with foregoing oil phase dispersion problem, if can design a kind of surface is organosilane, kernel is SiO
2silicon ball, by suitable etching reagent, erode kernel, just can obtain a kind of nano-hollow ball of surface hydrophobicity.Expand the preparation method of nano-hollow ball by this method, obtained the hydrophobic hollow ball of a kind of rich surface containing organic group, add its oil phase dispersed.For medicament slow release, support of the catalyst, pollute absorption, atmosphere storage etc. provide the selection of more horn of plenty.
Summary of the invention
The object of the present invention is to provide a kind of dewatering nano silicon oxide hollow ball material of organic decoration.This hollow ball material can be medicament slow release, support of the catalyst, and pollute absorption, atmosphere storage etc. provide new selection.
Another object of the present invention is to provide the method preparing above-mentioned nano material.The method is easy and simple to handle, is easy to large batch of preparation, belongs to original method.
For achieving the above object, the technical solution used in the present invention is:
A dewatering nano silicon oxide hollow ball for organic decoration, with the Nano-meter SiO_2 of organic decoration
2solid sphere is presoma, with mineral acids such as hydrochloric acid for etching reagent, prepares dewatering nano silicon oxide hollow ball by the mode of corrosion.It can adopt general formula OgHS to represent, Og is one or more in methyl, ethyl, propyl group, vinyl, dodecyl base, octyl group, hexadecyl, naphthyl, phenyl, trifluoro propyl, pentafluorophenyl group.HS is HollowSilica.
The preparation of the dewatering nano silicon oxide hollow ball of described organic decoration can be done according to the following steps:
1) by the ammoniacal liquor of tensio-active agent, mass concentration 25-28%, water, organic phase and cosurfactant mixing composition reverse micro emulsion A; Adopt tetraethoxy and organosilane to be silicon source, be mixed and made into solution B; Under the condition stirred, solution B is added in solution A, and aging 2-48h; The mass ratio of the final mixing solutions of gained is, 1 ~ 8 part of tensio-active agent: 1 ~ 4 part of water: 0.05 ~ 2 part of ammonia; 5 ~ 9 parts of organic phases: 1 ~ 6 portion of cosurfactant: 1 part of tetraethoxy: 0.05 ~ 1.5 part of organosilane;
2) the 1-20 ethanol breakdown of emulsion doubly of silicon source quality is added, collected by centrifugation solid; The ethanol adding 5-50 times of silicon source quality, under room temperature to reflux temperature, washs the tensio-active agent that 2-6 time is removed solid surface, 80-150 DEG C of oven dry.
3) get dried solid, add the 5-20 small molecular alcohol doubly of solid masses, ultrasonic 0.5-6h, adds the inorganic acid solution that massfraction is 0.5-40%, and stir 1-24h, collected by centrifugation solid, washes 1-6 time with deionized water, dries and both obtains.
Due to tensio-active agent, the kind of cosurfactant and organic phase can affect the pattern of nano material, described tensio-active agent is C8-20 linear alkylbenzene sulphonic acid in anion surfactant or α-sodium olefin sulfonate, or be the organic primary amine of C8-20 long-chain in nonionogenic tenside, Np series or TWEEN Series tensio-active agent, or be the hexadecyl trimethyl ammonium bromide in cats product; Described organic phase is hexanaphthene, normal hexane or toluene; Cosurfactant is propyl carbinol, Pentyl alcohol, n-hexyl alcohol or n-Octanol.
Because the diameter of the dewatering nano silicon oxide hollow ball of described organic decoration and the size of cavity directly can affect the specific surface of this material, therefore the diameter of described hollow ball is 10-300 nanometer, and wall thickness is 2-30 nanometer.
Because the kind of the organic group of silicon ball surface and quantity can be dispersed to the oil phase of silicon ball, catalytic performance, pollute absorption etc. to have an impact, therefore be methyltrimethoxy silane in described organosilane, ethyl trimethoxy silane, propyl trimethoxy silicane, vinyltrimethoxy silane, r-chloropropyl trimethoxyl silane, phenyltrimethoxysila,e, naphthyl Trimethoxy silane, dodecyltrimethoxysilane, octadecyl base Trimethoxy silane, trifluoro propyl Trimethoxy silane, one or more in pentafluorophenyl group Trimethoxy silane and corresponding Ethoxysilane thereof.The mass content of organic group in OgHS is 0.5-50%.
Process small molecular alcohol due to corrosion can affect the speed of corrosion, the size of the inner chamber of hollow ball and the specific surface of hollow ball that formed after corrosion, therefore described small molecular alcohol is one or more in methyl alcohol, ethanol, Virahol, n-propyl alcohol, propyl carbinol and isopropylcarbinol.
Because different mineral acids is for the corrosion speed of silicon ball, hollow ball be formed with important effect, described mineral acid comprise in hydrochloric acid, hydrofluoric acid, Hydrogen bromide, hydroiodic acid HI, sulfuric acid, nitric acid, phosphoric acid, boric acid one or more.
The present invention has the following advantages:
The hollow ball homogeneous grain diameter obtained, size controlled (see Fig. 1, Fig. 2).
The cavity of the hollow ball of gained is even, and specific surface area large (Fig. 4), hydrophobic angle are high, oil phase good dispersity (Fig. 3), and at medicament slow release, catalytic carrier, gas storage, pollutes the aspects such as absorption and have broad application prospects.
Accompanying drawing explanation
Fig. 1 is the TEM picture of dewatering nano silicon oxide hollow ball PhHS.
The size distribution of Fig. 2 PhHS.
The contact angle of Fig. 3 PhHS.
The nitrogen adsorption curve of Fig. 4 PhHS.
Embodiment
The following example will contribute to understanding the present invention, but content of the present invention is not limited thereto.
The preparation of embodiment 1 materials A (EtHS)
Get 15.5gNp-12,25g toluene, the ammoniacal liquor of 2g mass concentration 25% ~ 28%, 5.5g water and 3g propyl carbinol are mixed to get solution A; 1g tetraethoxy and 0.5g ethyl trimethoxy silane are mixed into B; Under vigorous stirring, solution B is joined in A and go, vigorous stirring 30min, aging 24h, add 20mL ethanol, centrifugally obtain white solid.In this solid, add 50mL ethanol, be heated to 40 DEG C and stir 10min, collected by centrifugation solid, repeats 6 times, until impurity removing.80 DEG C of dry 12h.The white solid obtained is joined in 80mL ethanol, ultrasonic 1h.Add the hydrochloric acid of 10mL mass concentration 4%, stir 12h.Centrifugally obtain white solid, wash 3 times, use 20mL ethanol at every turn.80 DEG C of dry 12h both obtained EtHS.
The preparation of embodiment 2 material B-E
The same materials A of preparation method of material B-E, difference is organosilane, and in the kind of small molecular alcohol and mineral acid, concrete kind is in table 1, and table 1 listed in by the material obtained
The organosilane, small molecular alcohol and the mineral acid kind that adopt in prepared by table 1 material B-E
Embodiment 3 material F(DoHS) preparation
Get 20gNp-7,15g hexanaphthene, the ammoniacal liquor of 1g25% ~ 28%, 7.5g water and 3g n-hexyl alcohol are mixed to get solution A; 2g tetraethoxy and 0.4g dodecyltrimethoxysilane are mixed into B; Under vigorous stirring, solution B is joined in A and go, vigorous stirring 30min, aging 8h, add 20mL ethanol, centrifugally obtain white solid.In this solid, add 50mL ethanol, be heated to 50 DEG C and stir 10min, centrifugal, repeat 6 times, until impurity removing.80 DEG C of dry 12h.The white solid obtained is joined in 80mL methyl alcohol, ultrasonic 1h.Add the hydrofluoric acid of 10mL4%, stir 2h.Centrifugally obtain white solid, wash 3 times, use 20mL ethanol at every turn.80 DEG C of dry 12h both obtained DoHS.
The preparation of embodiment 4 material G-J
The preparation method of material G-J is with material F, and difference is organosilane, and in the kind of small molecular alcohol and mineral acid, the concrete kind that adopts is in table 2, and table 2 listed in by the material obtained
The organosilane, small molecular alcohol and the mineral acid kind that adopt in prepared by table 1 material G-J
The hollow ball homogeneous grain diameter that the method obtains, size are controlled, and hydrophobic angle is high, are medicament slow release, support of the catalyst, and pollute absorption, atmosphere storage etc. provide the selection of more horn of plenty.
Claims (8)
1. a preparation method for organic decoration dewatering nano silicon oxide hollow ball, is characterized in that: operate in accordance with the following steps:
1) by the ammoniacal liquor of tensio-active agent, mass concentration 25-28%, water, organic phase and cosurfactant mixing composition reverse micro emulsion A; Adopt tetraethoxy and other organosilane I to be silicon source, be mixed and made into solution B; Under the condition stirred, solution B is added in solution A, and aging 2-48h; The mass ratio of the final mixing solutions of gained is, 1 ~ 8 part of tensio-active agent: 1 ~ 4 part of water: 0.05 ~ 2 part of ammonia: 5 ~ 9 parts of organic phases: 1 ~ 6 portion of cosurfactant: 1 part of tetraethoxy: 0.05 ~ 1.5 part of organosilane I;
2) the 1-20 ethanol breakdown of emulsion doubly of silicon source quality is added, collected by centrifugation solid; The 5-50 ethanol doubly adding silicon source quality is heated to room temperature to the washing that refluxes, and collects solid, repeated washing process 2-6 time, collects solid 80-150 DEG C oven dry;
3) get dried solid, add the 5-20 C1-C4 small molecular alcohol doubly of solid masses, ultrasonic 0.5-6h, add the inorganic acid solution of 1 ~ 20 times of mass concentration 0.5-40% of solid masses again, stir 1-24h, collected by centrifugation solid, wash 1-6 time with deionized water, dry and obtain OgHS;
The Nano-meter SiO_2 of the organic decoration obtained with microemulsion method
2solid sphere presoma, with mineral acids such as hydrochloric acid for etching reagent, prepares hollow nano silicon ball by the mode of chemical corrosion; Adopt general formula OgHS to represent, Og is one or more in methyl, ethyl, propyl group, vinyl, dodecyl, octyl group, hexadecyl, naphthyl, phenyl, trifluoro propyl and pentafluorophenyl group; HS is HollowSilica.
2. according to preparation method according to claim 1, it is characterized in that: described tensio-active agent is C8-20 linear alkylbenzene sulphonic acid in anion surfactant or α-sodium olefin sulfonate, or be the organic primary amine of C8-20 long-chain in nonionogenic tenside, Np series or TWEEN Series tensio-active agent, or be the hexadecyl trimethyl ammonium bromide in cats product; Described organic phase is hexanaphthene, normal hexane or toluene; Cosurfactant is propyl carbinol, Pentyl alcohol, n-hexyl alcohol or n-Octanol.
3. according to preparation method according to claim 1, it is characterized in that: described organosilane I is one in methyltrimethoxy silane, ethyl trimethoxy silane, propyl trimethoxy silicane, vinyltrimethoxy silane, r-chloropropyl trimethoxyl silane, phenyltrimethoxysila,e, naphthyl Trimethoxy silane, dodecyltrimethoxysilane, octadecyl trimethoxysilane, trifluoro propyl Trimethoxy silane, pentafluorophenyl group Trimethoxy silane and corresponding Ethoxysilane thereof or more than two kinds.
4. according to preparation method according to claim 1, it is characterized in that: described small molecular alcohol is one in methyl alcohol, ethanol, Virahol, n-propyl alcohol, propyl carbinol and isopropylcarbinol or more than two kinds.
5. according to preparation method according to claim 1, it is characterized in that: described mineral acid comprises one in hydrochloric acid, hydrofluoric acid, Hydrogen bromide, hydroiodic acid HI, sulfuric acid, nitric acid, phosphoric acid and boric acid or two or more.
6. the dewatering nano silicon oxide hollow ball of organic decoration for preparing of the arbitrary described method of claim 1-5.
7. according to hollow ball according to claim 6, it is characterized in that: the diameter of described hollow nano silicon ball is 10-300 nanometer, and wall thickness is 2-30 nanometer.
8. according to hollow ball according to claim 6, it is characterized in that: the mass content of organic group in OgHS is 0.5-50%.
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| CN108654684B (en) * | 2017-03-29 | 2020-09-04 | 中国科学院大连化学物理研究所 | B/L acid modified organic silicon ball catalyst, preparation and application thereof |
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